From 38ffeb8e94151137dca31598818f8434fe16aab1 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Thu, 19 Jun 2025 23:15:00 +0800 Subject: [PATCH 1/4] example PD_QPA_INTERNAL_STD --- cif_pow.dic | 53 +++++++++++++++++++++++++++++++++++++++++++++++++++-- 1 file changed, 51 insertions(+), 2 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index 2f4a2c25..fa34cb6a 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -11842,7 +11842,7 @@ save_PD_QPA_INTERNAL_STD _definition.id PD_QPA_INTERNAL_STD _definition.scope Category _definition.class Set - _definition.update 2023-01-16 + _definition.update 2025-06-19 _description.text ; This category identifies the internal standard used for @@ -11878,6 +11878,55 @@ save_PD_QPA_INTERNAL_STD '_pd_qpa_internal_std.diffractogram_id' '_pd_qpa_internal_std.phase_id' + _description_example.case +; + _audit.schema Custom + _pd_diffractogram.id DIFFRACTOGRAM_1 + + loop_ + _pd_phase_mass.phase_id + _pd_phase_mass.absolute + _pd_phase_mass.absolute_su + PHASE_1 42.81 0.56 + PHASE_2 14.73 0.24 + NIST_ALUMINA_676A 24.76 0.28 + + _pd_qpa_internal_std.mass_percent 25.000 + _pd_qpa_internal_std.mass_percent_su 0.002 + _pd_qpa_internal_std.crystallinity_percent 99.02 + _pd_qpa_internal_std.crystallinity_percent_su 1.11 + _pd_qpa_internal_std.phase_id NIST_ALUMINA_676A + + _pd_qpa_overall.method ZMV +; + _description_example.detail +; + A diffraction pattern containing three phases (PHASE_1, PHASE_2, and + some NIST SRM646a) has been quantified using the ZMV algorithm after + Rietveld refinement. + + The diffraction pattern was collected from a specimen containing + 25.000 ± 0.002 wt% internal standard (i.e. 1 g added to 3 g of unknown + to make a specimen with total weight of 4 g). The internal standard is + known to be 99.02 ± 1.11 % crystalline, and so the reported value of + _pd_phase_mass.percent for the standard is 25.000 * 0.9902 = 24.96 wt%. + + The weight fractions derived from the ZMW algorithm were then scaled as + + W~p~^absolute^ = W~p~^ZMV^ * (W~s~^known^ / W~s~^ZMV^) + + where W is the weight percentage, p is the phase, s is the standard + 'ZMV' is the weight fraction from the ZMV algorithm, and 'known' is the + known addition of standard (_pd_qpa_internal_std.mass_percent). These + are the values reported as _pd_phase_mass.absolute. Any difference + between the sum of the _pd_phase_mass.absolute values and 100 wt% can + be attributed to unanalysed or amorphous phases. + + The crystal structure of the internal standard is described by the + information linked to the _pd_phase.id data item with the value + 'NIST_ALUMINA_676A'. +; + save_ save_pd_qpa_internal_std.crystallinity_percent @@ -13102,7 +13151,7 @@ save_ Added examples to PD_CALC_OVERALL, PD_CALIB_INCIDENT_INTENSITY, PD_CHAR, _pd_diffractogram.id, PD_PEAK, _pd_phase.id, PD_PHASE_MASSS, PD_PREP, - PD_PROC_LS, PD_QPA_CALIB_FACTOR, PD_SPEC. + PD_PROC_LS, PD_QPA_CALIB_FACTOR, PD_QPA_INTERNAL_STD, PD_SPEC. PD_CALIB_WAVELENGTH removed. _diffrn_radiation_wavelength.phase_id and _diffrn_radiation_wavelength.diffractogram_id added to record From ee22f529bd025da148f3025ce1bc0774524c5740 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Fri, 20 Jun 2025 19:58:03 +0800 Subject: [PATCH 2/4] clarifications --- cif_pow.dic | 4 ++-- 1 file changed, 2 insertions(+), 2 deletions(-) diff --git a/cif_pow.dic b/cif_pow.dic index fa34cb6a..6677b30f 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -11902,14 +11902,14 @@ save_PD_QPA_INTERNAL_STD _description_example.detail ; A diffraction pattern containing three phases (PHASE_1, PHASE_2, and - some NIST SRM646a) has been quantified using the ZMV algorithm after + some NIST SRM676a) has been quantified using the ZMV algorithm after Rietveld refinement. The diffraction pattern was collected from a specimen containing 25.000 ± 0.002 wt% internal standard (i.e. 1 g added to 3 g of unknown to make a specimen with total weight of 4 g). The internal standard is known to be 99.02 ± 1.11 % crystalline, and so the reported value of - _pd_phase_mass.percent for the standard is 25.000 * 0.9902 = 24.96 wt%. + _pd_phase_mass.absolute for the standard is 25.000 * 0.9902 = 24.76 wt%. The weight fractions derived from the ZMW algorithm were then scaled as From fdf4dc1512680113fdb1b9b6afa551cdc561f002 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Mon, 23 Jun 2025 18:44:37 +0800 Subject: [PATCH 3/4] layout --- cif_pow.dic | 3 ++- 1 file changed, 2 insertions(+), 1 deletion(-) diff --git a/cif_pow.dic b/cif_pow.dic index 6677b30f..3f2ab16d 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -11909,7 +11909,8 @@ save_PD_QPA_INTERNAL_STD 25.000 ± 0.002 wt% internal standard (i.e. 1 g added to 3 g of unknown to make a specimen with total weight of 4 g). The internal standard is known to be 99.02 ± 1.11 % crystalline, and so the reported value of - _pd_phase_mass.absolute for the standard is 25.000 * 0.9902 = 24.76 wt%. + _pd_phase_mass.absolute for the standard is: + 25.000 * 0.9902 = 24.76 wt%. The weight fractions derived from the ZMW algorithm were then scaled as From a86bd6c70bdba819a5b6d582e1af97f077ee5505 Mon Sep 17 00:00:00 2001 From: Matthew Rowles Date: Thu, 26 Jun 2025 19:24:23 +0800 Subject: [PATCH 4/4] speeling --- cif_pow.dic | 2 +- 1 file changed, 1 insertion(+), 1 deletion(-) diff --git a/cif_pow.dic b/cif_pow.dic index 3f2ab16d..3e4bedbf 100644 --- a/cif_pow.dic +++ b/cif_pow.dic @@ -11912,7 +11912,7 @@ save_PD_QPA_INTERNAL_STD _pd_phase_mass.absolute for the standard is: 25.000 * 0.9902 = 24.76 wt%. - The weight fractions derived from the ZMW algorithm were then scaled as + The weight fractions derived from the ZMV algorithm were then scaled as W~p~^absolute^ = W~p~^ZMV^ * (W~s~^known^ / W~s~^ZMV^)